Liquid-solid cyclone separator, application thereof and method for removing solid-phase catalyst from copolymer solution

Abstract

The invention relates to the field of removal of a solid-phase catalyst from a copolymer solution, and discloses a liquid-solid cyclone separator, application of the liquid-solid cyclone separator and a method for removing the solid-phase catalyst from the copolymer solution. The liquid-solid cyclone separator comprises a cylindrical part and a conical part, and the cylindrical part is provided with a material inlet pipe and an overflow pipe; the conical part is provided with an underflow pipe; the material inlet pipe is tangentially arranged at the upper part of the cylindrical part; and the diameter of the material inlet pipe is gradually reduced in the horizontal direction from the part far away from the cylindrical part to the part in contact with the circular barrel. The liquid-solid cyclone separator can realize efficient separation of a solid-phase catalyst.

Description

Technical Field

[0001] The present invention relates to the field of removing solid-phase catalysts from copolymer solutions. Specifically, it relates to a liquid-solid cyclone separator, its application, and a method for removing solid-phase catalysts from copolymer solutions. Background Art

[0002] The polybutadiene segment in styrene-butadiene block copolymer contains double bonds, which greatly limits its aging resistance and weather resistance. Usually, homogeneous hydrogenation technology can be used to saturate the hydrogenation of the polybutadiene segment therein, thereby significantly improving its aging resistance and weather resistance. When using a heterogeneous catalyst for the full hydrogenation of styrene-butadiene block copolymer, usually at a certain reaction pressure and temperature, a solid-phase metal catalyst is added to the styrene-butadiene block copolymer solution, so that the double bonds in the C6 ring and the butadiene segment in the block copolymer undergo a full hydrogenation reaction. During the entire hydrogenation reaction process, the solid-phase metal catalyst is suspended in the copolymer solution, so the material system is in a slurry state. After the full hydrogenation reaction is completed, in order to ensure the transparency of the hydrogenated block copolymer product and recover the expensive catalyst, the solid-phase metal catalyst needs to be removed from the copolymer solution.

[0003] In the prior art, traditional methods for separating solid-phase catalysts from slurry systems usually include natural sedimentation method, filtration method, centrifugation method, etc. Among them, the natural sedimentation method has poor separation effect when the particle size is very small; the filtration method is prone to blockage of the filtration medium; the centrifugal separation method has large investment and high equipment maintenance cost.

[0004] To solve the problems existing in the traditional technology, CN213202926U discloses a catalytic cracking slurry desolidification device, which solves the problem of easy blockage caused by using a large number of small-particle-size fillers in the original solid-liquid separator; the device drives the rotating shaft to rotate through a driving motor, the rotating shaft drives the crankshaft to rotate, drives the connecting rod to move through the set bushing, and the connecting rod pulls the packing box to shake through the vertical plate, so that the material blocked in the through hole is discharged, thereby achieving the effect of anti-blocking. CN107497373A discloses a device for separating catalysts in slurry. By arranging a rotating drum inside the device housing, the accommodation space between the outer surface of the rotating drum and the inner surface of the housing is sequentially divided into a magnetic separation area, an elution drying area, and a demagnetization stripping area according to the rotation direction of the rotating drum. Under the action of the rotating drum, the catalyst is first attached to the outer surface of the rotating drum, and then to the elution drying area and the demagnetization stripping area, thereby realizing the separation of the catalyst in the slurry. However, the improved scheme is still difficult to obtain a hydrogenated block copolymer product with an extremely low content of solid-phase catalyst, and the equipment is complex, difficult to manufacture, and has strict requirements for the operation and control of the catalyst removal process. Summary of the Invention

[0005] The object of the present invention is to overcome the problems that the content of the solid-phase catalyst remaining in the copolymer solution is relatively high and the equipment for removing the solid-phase catalyst is complex, and to provide a liquid-solid cyclone separator, its application, and a method for removing the solid-phase catalyst from the copolymer solution. The structure of the liquid-solid cyclone separator is simple, which can achieve efficient separation between the solid-phase catalyst and the copolymer solution, and can obtain a copolymer product with an extremely low content of the solid-phase catalyst.

[0006] To achieve the above object, the first aspect of the present invention provides a liquid-solid cyclone separator, wherein the liquid-solid cyclone separator includes a cylindrical part and a conical part. The cylindrical part is provided with a material inlet pipe and an overflow pipe, and the conical part is provided with an underflow pipe;

[0007] The material inlet pipe is tangentially arranged at the upper part of the cylindrical part;

[0008] Along the horizontal direction from far away from the cylindrical part to contacting the circular cylinder, the diameter of the material inlet pipe shows a decreasing trend.

[0009] The second aspect of the present invention provides an application of the above liquid-solid cyclone separator in separating the solid phase from the liquid phase.

[0010] The third aspect of the present invention provides a method for removing the solid-phase catalyst from the copolymer solution, wherein the method uses the above liquid-solid cyclone separator.

[0011] Through the above technical solutions, the liquid-solid cyclone separator, its application, and the method for removing the solid-phase catalyst from the copolymer solution provided by the present invention have the following beneficial effects.

[0012] In the present invention, by tangentially arranging the material inlet pipe at the upper part of the cylindrical part and making the diameter of the material inlet pipe gradually decrease along the horizontal direction from far away from the cylindrical part to contacting the circular cylinder, the centrifugal force of the copolymer solution in the liquid-solid cyclone separator is increased, thereby realizing the efficient separation of the solid-phase catalyst. The liquid-solid cyclone separator is a static device with a simple structure, which is easy to process, manufacture, and maintain.

[0013] By using the liquid-solid cyclone separator to remove the solid-phase catalyst from the copolymer solution, a copolymer product with an extremely low content of the solid-phase catalyst can be obtained. Description of the Drawings

[0014] Figure 1 It is a schematic diagram of the liquid-solid cyclone separator of Example 1.

[0015] Figure 2 It is a top view of the liquid-solid cyclone separator of Example 1.

[0016] Description of the Reference Numerals

[0017] 1 - Cylindrical part; 2 - Conical part; 3 - Material inlet pipe; 4 - Overflow pipe; 5 - Spiral guide vane; 6 - Underflow pipe. Detailed implementation manner

[0018] The endpoints and any values within the ranges disclosed herein are not limited to the exact ranges or values. These ranges or values should be understood to include values close to these ranges or values. For numerical ranges, the endpoint values of each range, between the endpoint values of each range, between the endpoint values of each range and individual point values, and between individual point values can be combined with each other to obtain one or more new numerical ranges, and these numerical ranges should be regarded as specifically disclosed herein.

[0019] The first aspect of the present invention provides a liquid-solid cyclone separator, wherein the liquid-solid cyclone separator includes a cylindrical part and a conical part. The cylindrical part is provided with a material inlet pipe and an overflow pipe, and the conical part is provided with an underflow pipe;

[0020] The material inlet pipe is tangentially arranged at the upper part of the cylindrical part;

[0021] Along the horizontal direction from far away from the cylindrical part to contacting the circular cylinder, the diameter of the material inlet pipe shows a decreasing trend.

[0022] In the present invention, by tangentially arranging the material inlet pipe at the upper part of the cylindrical part and making the diameter of the material inlet pipe gradually decrease along the horizontal direction from far away from the cylindrical part to contacting the circular cylinder, the centrifugal force of the copolymer solution in the liquid-solid cyclone separator is increased, and thus the efficient separation of the solid-phase catalyst is realized. This liquid-solid cyclone separator is a static device, and has a simple structure, and is easy to process, manufacture and maintain.

[0023] In the present invention, the copolymer solution enters the liquid-solid cyclone separator from the material inlet pipe in the tangential direction of the cylindrical part. The copolymer solution generates a strong centrifugal force through its own rotational motion. The solid-phase catalyst suspended in the copolymer solution is thrown towards the wall of the separator under the action of the centrifugal force and flows downward along the wall of the separator, and flows out through the underflow pipe; the copolymer solution from which the solid-phase catalyst has been removed flows out from the overflow pipe.

[0024] Further, the material inlet pipe is tangentially arranged at the top of the cylindrical part.

[0025] According to the present invention, along the horizontal direction from far away from the cylindrical part to contacting the circular cylinder, the contraction angle of the rectangular cross-section of the material inlet pipe is 5 - 45°.

[0026] In the present invention, when the contraction angle satisfies the above range, the flow rate of the material entering the liquid-solid cyclone separator is beneficial to the separation of liquid and solid, and the pressure drop is appropriate, avoiding the short-circuit phenomenon of the material.

[0027] Further, in the horizontal direction away from the cylindrical part to the contact circular cylinder, the contraction angle of the rectangular cross-section of the material inlet pipe is 10-30°.

[0028] According to the present invention, when the diameter of the cylindrical part is D, the maximum diameter of the material inlet pipe is 1 / 6D - 7 / 12D.

[0029] In the present invention, the material inlet pipe is a contraction pipe, and the maximum diameter of the material inlet pipe refers to the diameter of the end of the material inlet pipe away from the cylindrical part. When the maximum diameter of the material inlet pipe meets the above range, a good matching of flow velocity and pressure drop can be achieved at a certain throughput, which is beneficial to the liquid and solid obtaining an appropriate initial separation velocity when passing through the contraction section and entering the liquid-solid cyclone separator.

[0030] Further, when the diameter of the cylindrical part is D, the maximum diameter of the material inlet pipe is 1 / 4D - 5 / 12D.

[0031] According to the present invention, spiral guide vanes are provided on the outer wall of the overflow pipe.

[0032] In the present invention, the spiral guide vanes on the outer wall of the overflow pipe can cooperate with the material inlet pipe to increase the centrifugal force of the copolymer solution in the liquid-solid cyclone separator, which is beneficial to the efficient separation of the solid-phase catalyst from the copolymer solution.

[0033] According to the present invention, the overflow pipe is located at the top of the liquid-solid cyclone separator.

[0034] According to the present invention, the diameter of the overflow pipe is 1 / 5D - 7 / 12D.

[0035] In the present invention, when the diameter of the overflow pipe meets the above range, the requirement for the separation particle size of the solid-phase catalyst particles in the copolymer solution can be achieved, and the pressure drop is appropriate, so that the separated solid-phase catalyst can flow out smoothly.

[0036] Further, the diameter of the overflow pipe is 1 / 4D - 5 / 12D.

[0037] According to the present invention, the vertical insertion depth of the overflow pipe is 0.25D - 2D.

[0038] In the present invention, when the vertical insertion depth of the overflow pipe meets the above range, the separation accuracy of the solid-phase catalyst particles in the copolymer solution can be ensured, and the material entering the liquid-solid cyclone separator can be prevented from directly entering the overflow pipe and causing a short circuit.

[0039] Further, the vertical insertion depth of the overflow pipe is 0.5 - 1.5D.

[0040] According to the present invention, the underflow pipe is located at the bottom of the liquid-solid cyclone separator.

[0041] According to the present invention, the diameter of the underflow pipe is 1 / 6D - 7 / 12D.

[0042] In the present invention, when the diameter of the underflow pipe meets the above range, the separation accuracy and separation efficiency of the solid-phase catalyst particles in the copolymer solution can be taken into account.

[0043] Further, the diameter of the underflow pipe is 1 / 4D - 5 / 12D.

[0044] According to a preferred embodiment of the present invention, the maximum diameter of the material inlet pipe, the diameter of the overflow pipe, and the diameter of the underflow pipe are equal.

[0045] According to a preferred embodiment of the present invention, in the horizontal direction, the center of the overflow pipe and the center of the cylindrical part are on the same straight line.

[0046] According to the present invention, the pitch of the spiral guide vane is 0.2 - 1.5 times the diameter of the overflow pipe.

[0047] In the present invention, when the pitch of the spiral guide vane and the diameter of the overflow pipe meet the above relationship, it can promote the incoming material to flow along the central axis of the liquid-solid cyclone separator, increase the centrifugal force for the solid particles to be thrown out, and at the same time extend the liquid-solid separation path, thereby improving the liquid-solid separation effect.

[0048] Further, the pitch of the spiral guide vane is 0.5 - 1 times the diameter of the overflow pipe.

[0049] In the present invention, in the vertical direction, the included angle β formed by the outer wall of the conical part after extension is the cone angle. In order to further improve the separation accuracy and separation efficiency of the solid-phase catalyst in the copolymer solution, the value of the cone angle β is 2 - 45°, preferably 5 - 30°.

[0050] The following combines Figure 1 to illustrate the liquid-solid cyclone separator of the present invention. Specifically, the liquid-solid cyclone separator includes: a cylindrical part 1, a conical part 2, a material inlet pipe 3, an overflow pipe 4, a spiral guide vane 5, and an underflow pipe 6. The upper half of the liquid-solid cyclone separator is a cylindrical part. The material inlet pipe is tangentially arranged at the upper part of the cylindrical part. The overflow pipe is arranged at the top of the cylindrical part and extends downward into the cylindrical interior. The outer wall of the overflow pipe is provided with a spiral guide vane. The lower half of the liquid-solid cyclone separator is a conical part, and an underflow pipe is provided at the lower end of the conical part.

[0051] The following combines Figure 2The top view of the liquid-solid cyclone separator will be described. Specifically, the material inlet is tangentially arranged in the cylindrical part, and along the horizontal direction from the cylindrical part to the contact with the circular cylinder, the diameter of the material inlet pipe decreases; the contraction angle of the rectangular cross-section of the material inlet pipe is α, and the included angle β formed by the extension of the outer wall of the conical part is the cone angle; the diameter of the cylindrical part is D. The overflow pipe is arranged at the top of the cylindrical part.

[0052] The operation mode of the liquid-solid cyclone separator of the present invention is as follows: the copolymer solution material inlet pipe enters the liquid-solid cyclone separator in the tangential direction of the cylindrical part. At the maximum diameter of the material inlet pipe, the flow rate of the copolymer solution is 0.5 - 2.5 m / s. The spiral guide vanes on the contracted material inlet pipe and the overflow pipe cooperate to increase the centrifugal force of the copolymer solution in the liquid-solid cyclone separator. After cyclone separation, the solution containing the solid-phase catalyst flows out from the underflow pipe, and the nearly clarified hydrogenated copolymer solution flows out from the overflow pipe at the top.

[0053] The second aspect of the present invention provides an application of the above liquid-solid cyclone separator in separating solid phase from liquid phase.

[0054] Furthermore, the application of the liquid-solid cyclone separator in separating solid-phase catalyst from liquid-phase copolymer.

[0055] The third aspect of the present invention provides a method for removing solid-phase catalyst from copolymer solution, wherein the method uses the above liquid-solid cyclone separator.

[0056] In the present invention, by removing the solid-phase catalyst from the copolymer solution through the liquid-solid cyclone separator, a copolymer product with extremely low solid-phase catalyst content can be obtained.

[0057] According to the present invention, the copolymer solution is prepared by subjecting a pre-hydrogenated copolymer solution to a hydrogenation reaction of the solid-phase catalyst.

[0058] According to the present invention, the pre-hydrogenated copolymer is selected from at least one of styrene-butadiene copolymer, styrene-isoprene copolymer, and styrene-cyclopentadiene copolymer, and is preferably styrene-butadiene copolymer.

[0059] Furthermore, the pre-hydrogenated copolymer is styrene-butadiene copolymer.

[0060] According to the present invention, in the pre-hydrogenated copolymer, the content of styrene structural units is 30 - 95 wt%.

[0061] In the present invention, in the pre-hydrogenated copolymer, the contents of butadiene structural units, isoprene structural units, and cyclopentadiene structural units are each independently 5 - 70 wt%.

[0062] According to the present invention, after the pre-hydrogenated copolymer is subjected to a hydrogenation reaction using a solid-phase catalyst, the sum of the unsaturated double bond contents is ≤ 5 wt%.

[0063] In the present invention, there are no special limitations on the hydrogenation reaction, and it can be a conventional hydrogenation method in the art. For example, the temperature of the hydrogenation reaction is 60 - 250 °C, and the time of the hydrogenation reaction is 2 - 10 h; the solid-phase catalyst can be selected from at least one of nickel metal catalysts, platinum metal catalysts, and rhodium metal catalysts.

[0064] According to the present invention, at 25 °C, the kinematic viscosity of the copolymer solution is 10 - 100 cP.

[0065] In the present invention, when the kinematic viscosity of the copolymer solution satisfies the above range, by using the liquid-solid cyclone separator of the present invention, a better separation effect can be obtained between the copolymer solution and the solid catalyst.

[0066] Further, at 25 °C, the kinematic viscosity of the copolymer solution is 30 - 80 cP.

[0067] According to the present invention, the content of the solid-phase catalyst in the copolymer solution is 3 - 10 wt%.

[0068] Further, the content of the solid-phase catalyst in the copolymer solution is 5 - 8 wt%.

[0069] According to the present invention, after the copolymer solution is subjected to removal of the solid-phase catalyst, the content of the solid-phase catalyst in the obtained hydrogenated copolymer solution is ≤ 9 ppm.

[0070] Further, after the copolymer solution is subjected to removal of the solid-phase catalyst, the content of the solid-phase catalyst in the obtained hydrogenated copolymer solution is ≤ 5 ppm.

[0071] In the present invention, at the maximum diameter of the material inlet pipe, the flow rate of the copolymer solution is 0.5 - 2.5 m / s.

[0072] The present invention will be described in detail below through examples.

[0073] In the following examples, the styrene monomer content, butadiene monomer content, and unsaturated double bond content are measured by nuclear magnetic resonance detection methods;

[0074] The kinematic viscosity (25 °C) of the copolymer solution is measured by a HAAKE rotational rheometer;

[0075] The styrene-butadiene block copolymer is synthesized by a solution method, wherein the content of the styrene structural unit is 65 wt%, and the content of the butadiene structural unit is 35 wt%.

[0076] Other raw materials used in the examples and comparative examples are all commercially available products.

[0077] Preparation Example 1

[0078] In a hydrogenation autoclave, 2 kg of styrene-butadiene was mixed with 105 g of a solid-phase catalyst (nickel metal catalyst). The content of the solid-phase catalyst in the styrene-butadiene solution was 5 wt%. At 100 °C, hydrogen was introduced and the hydrogenation reaction was carried out for 6 h to obtain a copolymer solution with an unsaturated double bond content of 2 wt% and a viscosity of 30 cP.

[0079] Example 1

[0080] The diameter D of the cylindrical section of the liquid-solid cyclone separator was 100 mm, the length of the cylindrical section was 200 mm, the height of the bottom conical section was 250 mm, and the cone angle was 20°. The contraction angle of the rectangular cross-section of the material inlet pipe was 10°. The maximum diameter of the material inlet pipe, the diameter of the overflow pipe, and the diameter of the underflow pipe were all 25 mm, that is, the maximum diameter of the material inlet pipe, the diameter of the overflow pipe, and the diameter of the underflow pipe were 1 / 4D. The vertical insertion depth of the overflow pipe was 50 mm (the vertical insertion depth of the overflow pipe was 0.5D), and the pitch of the spiral guide vanes on the outer wall of the overflow pipe was 12.5 mm (the pitch of the spiral guide vanes was 0.5 times the diameter of the overflow pipe).

[0081] The copolymer solution entered the liquid-solid cyclone separator at a flow rate of 2 m / s at the maximum diameter of the material inlet pipe. After cyclone separation, the solution containing the solid-phase catalyst flowed out from the underflow pipe, and the nearly clarified hydrogenated copolymer solution flowed out from the overflow pipe at the top. The material flowing out from the underflow pipe was dried and weighed in an oven to obtain the mass of the removed solid-phase catalyst, and then the content of the solid-phase catalyst in the hydrogenated copolymer solution after removing the solid-phase catalyst was calculated to be 3 ppm.

[0082] Example 2

[0083] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the contraction angle of the rectangular cross-section of the material inlet pipe was 20°. The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 2.7 ppm.

[0084] Example 3

[0085] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the contraction angle of the rectangular cross-section of the material inlet pipe was 30°. The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 2.5 ppm.

[0086] Example 4

[0087] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the maximum diameter of the material inlet pipe, the diameter of the overflow pipe, and the diameter of the underflow pipe were all 40 mm, that is, the maximum diameter of the material inlet pipe, the diameter of the overflow pipe, and the diameter of the underflow pipe were 0.4D. The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 4.6 ppm.

[0088] Example 5

[0089] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the maximum diameter of the material inlet pipe was 25 mm (i.e., the maximum diameter of the material inlet pipe was 1 / 4D), the diameter of the overflow pipe and the diameter of the underflow pipe were both 40 mm (i.e., the diameter of the overflow pipe and the diameter of the underflow pipe were 0.4D), and the flow rate of the copolymer solution entering the liquid-solid cyclone separator at the maximum diameter of the material inlet pipe was 2 m / s. The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 3.8 ppm.

[0090] Example 6

[0091] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the vertical insertion depth of the overflow pipe was 100 mm (the vertical insertion depth of the overflow pipe was 1D). The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 3.4 ppm.

[0092] Example 7

[0093] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the vertical insertion depth of the overflow pipe was 150 mm (the vertical insertion depth of the overflow pipe was 1.5D). The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 3.6 ppm.

[0094] Example 8

[0095] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the pitch of the spiral guide vane on the outer wall of the overflow pipe was 18.75 mm (the pitch of the spiral guide vane was 0.75 times the diameter of the overflow pipe). The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 3.2 ppm.

[0096] Example 9

[0097] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the pitch of the spiral guide vane on the outer wall of the overflow pipe was 25 mm (the pitch of the spiral guide vane was 1 times the diameter of the overflow pipe). The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 3.3 ppm.

[0098] Example 10

[0099] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that there were no spiral guide vanes on the outer wall of the overflow pipe. The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 9 ppm.

[0100] Example 11

[0101] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the contraction angle of the rectangular cross-section of the material inlet pipe was 35°. The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 4.6 ppm.

[0102] Example 12

[0103] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the contraction angle of the rectangular cross-section of the material inlet pipe was 3°. The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 4.8 ppm.

[0104] Example 13

[0105] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the maximum diameter of the material inlet pipe, the diameter of the overflow pipe, and the diameter of the underflow pipe were all 50 mm, that is, the maximum diameter of the material inlet pipe, the diameter of the overflow pipe, and the diameter of the underflow pipe were 0.5D. The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 4.9 ppm.

[0106] Example 14

[0107] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the maximum diameter of the material inlet pipe, the diameter of the overflow pipe, and the diameter of the underflow pipe were all 20 mm, that is, the maximum diameter of the material inlet pipe, the diameter of the overflow pipe, and the diameter of the underflow pipe were 0.2D. The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 4.8 ppm.

[0108] Example 15

[0109] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the pitch of the spiral guide vanes on the outer wall of the overflow pipe was 30 mm (the pitch of the spiral guide vanes was 1.2 times the diameter of the overflow pipe). The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 4 ppm.

[0110] Example 16

[0111] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the pitch of the spiral guide vanes on the outer wall of the overflow pipe was 10 mm (the pitch of the spiral guide vanes was 0.4 times the diameter of the overflow pipe). The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 3.8 ppm.

[0112] Example 17

[0113] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the contraction angle of the rectangular cross-section of the material inlet pipe was 3°, the diameters of the overflow pipe and the underflow pipe were both 60 mm (i.e., the diameters of the overflow pipe and the underflow pipe were 0.6D), and the pitch of the spiral guide vanes on the outer wall of the overflow pipe was 96 mm (the pitch of the spiral guide vanes was 3.8 times the diameter of the overflow pipe). The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 6.5 ppm.

[0114] Comparative Example 1

[0115] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the rectangular cross-section of the material inlet pipe did not contract. The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 9.5 ppm.

[0116] Comparative Example 2

[0117] The solid-phase catalyst in the copolymer solution was removed according to the method of Example 1, except that the contraction angle of the rectangular cross-section of the material inlet pipe was 0°, the diameters of the overflow pipe and the underflow pipe were both 10 mm (i.e., the diameters of the overflow pipe and the underflow pipe were 0.1D), and the pitch of the spiral guide vanes on the outer wall of the overflow pipe was 2.5 mm (the pitch of the spiral guide vanes was 0.1 times the diameter of the overflow pipe). The content of the solid-phase catalyst in the obtained hydrogenated copolymer solution was 10 ppm.

[0118] The preferred embodiments of the present invention have been described in detail above. However, the present invention is not limited thereto. Within the technical concept of the present invention, various simple modifications can be made to the technical solutions of the present invention, including any other suitable combination of each technical feature. These simple modifications and combinations should also be regarded as the content disclosed by the present invention and fall within the protection scope of the present invention.

Claims

1. A liquid-solid cyclone separator, characterized in that, The liquid-solid cyclone separator includes a cylindrical part (1) and a conical part (2). The cylindrical part (1) is provided with a material inlet pipe (3) and an overflow pipe (4), and the conical part (2) is provided with an underflow pipe (6). The material inlet pipe (3) is tangentially arranged at the upper part of the cylindrical part (1). Along the horizontal direction from far away from the cylindrical part (1) to contacting the cylindrical part (1), the diameter of the material inlet pipe (3) shows a decreasing trend.

2. The liquid-solid cyclone separator according to claim 1, wherein, The material inlet pipe (3) is tangentially arranged at the top of the cylindrical part (1). Preferably, along the horizontal direction from far away from the cylindrical part to contacting the cylindrical part, the contraction angle of the rectangular cross-section of the material inlet pipe (3) is 5 - 45°, preferably 10 - 30°.

3. The liquid-solid cyclone separator according to claim 1 or 2, wherein, When the diameter of the cylindrical part (1) is D, the maximum diameter of the material inlet pipe (3) is 1 / 6D - 7 / 12D, preferably 1 / 4D - 5 / 12D.

4. The liquid-solid cyclone separator according to any one of claims 1-3, wherein, The outer wall of the overflow pipe (4) is provided with spiral guide vanes (5). Preferably, the overflow pipe (4) is located at the top of the liquid-solid cyclone separator. Preferably, the diameter of the overflow pipe (4) is 1 / 5D - 7 / 12D, preferably 1 / 4D - 5 / 12D. Preferably, the vertical insertion depth of the overflow pipe (4) is 0.25D - 2D, preferably 0.5D - 1.5D.

5. The liquid-solid cyclone separator according to any one of claims 1-4, wherein, The underflow pipe (6) is located at the bottom of the liquid-solid cyclone separator. Preferably, the diameter of the underflow pipe (6) is 1 / 6D - 7 / 12D, preferably 1 / 4D - 5 / 12D. Preferably, the maximum diameter of the material inlet pipe (3), the diameter of the overflow pipe (4), and the diameter of the underflow pipe (6) are equal.

6. The liquid-solid cyclone separator according to claim 4 or 5, wherein The pitch of the spiral guide vanes (5) is 0.2 - 1.5 times the diameter of the overflow pipe (4), preferably 0.5 - 1 times.

7. Application of the liquid-solid cyclone separator according to any one of claims 1 - 6 in separating solid phase from liquid phase; Preferably, the application of the liquid-solid cyclone separator in separating solid catalyst from liquid-phase copolymer.

8. A method for removing a solid-phase catalyst from a copolymer solution, characterized in that, The method uses the liquid-solid cyclone separator according to any one of claims 1 - 6.

9. The method according to claim 8, wherein, The copolymer solution is obtained by subjecting a pre-hydrogenated copolymer solution to a hydrogenation reaction with a solid catalyst. Preferably, the pre-hydrogenated copolymer is selected from at least one of styrene-butadiene copolymer, styrene-isoprene copolymer, and styrene-cyclopentadiene copolymer, preferably styrene-butadiene copolymer.

10. The method according to claim 9, wherein, In the pre-hydrogenated copolymer, the content of styrene structural units is 30 - 95 wt%. Preferably, after the pre-hydrogenated copolymer undergoes a hydrogenation reaction with a solid catalyst, the sum of the contents of unsaturated double bonds ≤ 5 wt%.

11. The method according to any one of claims 8-10, wherein, At 25 °C, the dynamic viscosity of the copolymer solution is 10 - 100 cP, preferably 30 - 80 cP. Preferably, the content of the solid catalyst in the copolymer solution is 3 - 10 wt%, preferably 5 - 8 wt%. Preferably, after the solid catalyst is removed from the copolymer solution, the content of the solid catalyst in the obtained hydrogenated copolymer solution ≤ 9 ppm, preferably ≤ 5 ppm.

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